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1.
Anal Bioanal Chem ; 405(24): 7765-72, 2013 Sep.
Artículo en Inglés | MEDLINE | ID: mdl-23404130

RESUMEN

In recent years, near-infrared (NIR) hyperspectral imaging has proved its suitability for quality and safety control in the cereal sector by allowing spectroscopic images to be collected at single-kernel level, which is of great interest to cereal control laboratories. Contaminants in cereals include, inter alia, impurities such as straw, grains from other crops, and insects, as well as undesirable substances such as ergot (sclerotium of Claviceps purpurea). For the cereal sector, the presence of ergot creates a high toxicity risk for animals and humans because of its alkaloid content. A study was undertaken, in which a complete procedure for detecting ergot bodies in cereals was developed, based on their NIR spectral characteristics. These were used to build relevant decision rules based on chemometric tools and on the morphological information obtained from the NIR images. The study sought to transfer this procedure from a pilot online NIR hyperspectral imaging system at laboratory level to a NIR hyperspectral imaging system at industrial level and to validate the latter. All the analyses performed showed that the results obtained using both NIR hyperspectral imaging cameras were quite stable and repeatable. In addition, a correlation higher than 0.94 was obtained between the predicted values obtained by NIR hyperspectral imaging and those supplied by the stereo-microscopic method which is the reference method. The validation of the transferred protocol on blind samples showed that the method could identify and quantify ergot contamination, demonstrating the transferability of the method. These results were obtained on samples with an ergot concentration of 0.02% which is less than the EC limit for cereals (intervention grains) destined for humans fixed at 0.05%.


Asunto(s)
Grano Comestible/química , Alcaloides de Claviceps/análisis , Calidad de los Alimentos , Espectroscopía Infrarroja Corta , Alcaloides de Claviceps/química , Humanos
2.
Artículo en Inglés | MEDLINE | ID: mdl-21995816

RESUMEN

Thirteen laboratories participated in an inter-laboratory study to evaluate the method performance characteristics of a liquid chromatography-tandem mass spectrometric method (LC-MS/MS) for marine lipophilic shellfish toxins. Method performance characteristics were evaluated for mussel (Mytilus edulis), oyster (Crassostrea gigas) and cockle (Cerastoderma edule) matrices. The specific toxin analogues tested included okadaic acid (OA), dinophysistoxins-1 and -2 (DTX1, -2), azaspiracids-1, -2 and -3 (AZA1, -2, -3), pectenotoxin-2 (PTX2), yessotoxin (YTX), and 45-OH-yessotoxin (45-OH-YTX). The instrumental technique was developed as an alternative to the still widely applied biological methods (mouse or rat bioassay). Validation was conducted according to the AOAC-harmonised protocol for the design, conduct and interpretation of method-performance studies. Eight different test materials were sent as blind duplicates to the participating laboratories. Twelve laboratories returned results that were accepted to be included in the statistical evaluation. The method precision was expressed as HORRATs. For the individual toxins (except for 45-OH-YTX) HORRATs were found to be ≤1.8 (median HORRAT=0.8) in all tested materials. The recoveries of OA-, AZA- and YTX-group toxins were within the range of 80-108% and PTX2 was within the range of 62-93%. Based on the acceptable values for precision and recovery, it was concluded that the method is suitable for official control purposes to quantitatively determine OA/DTXs, AZAs, YTXs and PTX2 in shellfish.


Asunto(s)
Bivalvos/química , Cardiidae/química , Cromatografía Liquida/métodos , Toxinas Marinas/análisis , Espectrometría de Masas/métodos , Ostreidae/química , Animales , Bioensayo , Contaminación de Alimentos , Laboratorios , Ratones , Control de Calidad , Ratas , Mariscos/análisis , Espectrometría de Masa por Ionización de Electrospray
3.
Environ Sci Technol ; 45(20): 8965-73, 2011 Oct 15.
Artículo en Inglés | MEDLINE | ID: mdl-21853993

RESUMEN

Currently, there are no fast in vitro broad spectrum screening bioassays for the detection of marine toxins. The aim of this study was to develop such an assay. In gene expression profiling experiments 17 marker genes were provisionally selected that were differentially regulated in human intestinal Caco-2 cells upon exposure to the lipophilic shellfish poisons azaspiracid-1 (AZA1) or dinophysis toxin-1 (DTX1). These 17 genes together with two control genes were the basis for the design of a tailored microarray platform for the detection of these marine toxins and potentially others. Five out of the 17 selected marker genes on this dedicated DNA microarray gave clear signals, whereby the resulting fingerprints could be used to detect these toxins. CEACAM1, DDIT4, and TUBB3 were up-regulated by both AZA1 and DTX1, TRIB3 was up-regulated by AZA1 only, and OSR2 by DTX1 only. Analysis by singleplex qRT-PCR revealed the up- and down-regulation of the selected RGS16 and NPPB marker genes by DTX1, that were not envisioned by the new developed dedicated array. The qRT-PCR targeting the DDIT4, RSG16 and NPPB genes thus already resulted in a specific pattern for AZA1 and DTX1 indicating that for this specific case qRT-PCR might a be more suitable approach than a dedicated array.


Asunto(s)
Toxinas Marinas/toxicidad , Análisis de Secuencia por Matrices de Oligonucleótidos/métodos , Antígenos CD/genética , Células CACO-2 , Moléculas de Adhesión Celular/genética , Expresión Génica/efectos de los fármacos , Perfilación de la Expresión Génica , Humanos , Ácido Ocadaico/análogos & derivados , Piranos/toxicidad , Reacción en Cadena de la Polimerasa de Transcriptasa Inversa , Compuestos de Espiro/toxicidad , Factores de Transcripción/genética , Tubulina (Proteína)/genética
4.
Artículo en Inglés | MEDLINE | ID: mdl-21360378

RESUMEN

Pyrrolizidine alkaloids are toxins present in many plants belonging to the families of Asteraceae, Boraginaceae and Fabaceae. Particularly notorious are pyrrolizidine alkaloids present in ragwort species (Senecio), which are held responsible for hepatic disease in horses and cows and may lead to the death of the affected animals. In addition, these compounds may be transferred to edible products of animal origin and as such be a threat for the health of consumers. To investigate the possible transfer of pyrrolizidine alkaloids from contaminated feed to milk, cows were put on a ration for 3 weeks with increasing amounts (50-200 g day(-1)) of dried ragwort. Milk was collected and sampled twice a day; faeces and urine twice a week. For milk, a dose-related appearance of pyrrolizidine alkaloids was found. Jacoline was the major component in milk despite being a minor component in the ragwort material. Practically no N-oxides were observed in milk, notwithstanding the fact that they constituted over 80% of the pyrrolizidine alkaloids in ragwort. The overall carry-over of the pyrrolizidine alkaloids was estimated to be only around 0.1%, but for jacoline 4%. Notwithstanding the low overall carry-over, this may be relevant for consumer health considering the genotoxic and carcinogenic properties demonstrated for some of these compounds. Analysis of the faeces and urine samples indicated that substantial metabolism of pyrrolizidine alkaloids is taking place. The toxicity and potential transfer of metabolites to milk is unknown and remains to be investigated.


Asunto(s)
Alimentación Animal/análisis , Bovinos/metabolismo , Leche/química , Alcaloides de Pirrolicidina/análisis , Alcaloides de Pirrolicidina/farmacocinética , Animales , Cromatografía Liquida , Heces/química , Femenino , Contaminación de Alimentos/análisis , Alcaloides de Pirrolicidina/orina , Senecio/química , Espectrometría de Masas en Tándem
5.
Eur J Clin Nutr ; 64(5): 534-40, 2010 May.
Artículo en Inglés | MEDLINE | ID: mdl-20234383

RESUMEN

BACKGROUND/OBJECTIVES: Acrylamide, a probable human carcinogen, was detected in various heat-treated foods such as French fries and potato crisps. Recently, positive associations have been found between dietary acrylamide intakes, as estimated with a food frequency questionnaire using an acrylamide database, and cancer risk in some epidemiological studies. As acrylamide levels vary considerably within the same type of foods, a validation study was performed to investigate whether use of an acrylamide food database containing calculated mean acrylamide content, based on extensive sampling and chemical analysis of Dutch foods (several samples per food), can classify subjects with respect to true acrylamide intake. SUBJECTS/METHODS: We used the data from a 24-h duplicate diet study. The acrylamide content of 39 Dutch 24-h duplicate diets collected in 2004 was estimated using the mean acrylamide levels of foods available from the database and the menu list, on which the participants of the duplicate diet study had listed the amounts of individual foods and drinks in household units. Next, the acrylamide content of the total duplicate diets was analytically measured and correlated to the estimated acrylamide contents. RESULTS: The Spearman's correlation coefficient between chemically determined acrylamide content and the calculated acrylamide content of the duplicate diets was 0.82 (P<0.001). CONCLUSIONS: This study indicates that it is possible to classify subjects with respect to acrylamide intake if mean instead of actual content of each food is applied. The database can therefore be applied in epidemiological studies on acrylamide intake and cancer risk, such as the Netherlands Cohort Study on Diet and Cancer.


Asunto(s)
Acrilamida/análisis , Carcinógenos/análisis , Bases de Datos Factuales , Dieta/clasificación , Estudios Epidemiológicos , Análisis de los Alimentos , Acrilamida/administración & dosificación , Adolescente , Adulto , Anciano , Carcinógenos/administración & dosificación , Femenino , Humanos , Masculino , Persona de Mediana Edad , Neoplasias/epidemiología , Países Bajos , Estadísticas no Paramétricas , Adulto Joven
6.
Food Addit Contam ; 23(10): 1008-20, 2006 Oct.
Artículo en Inglés | MEDLINE | ID: mdl-16982523

RESUMEN

An experiment was carried out to examine the effects of feeding Fusarium toxin-contaminated wheat (8.21 mg deoxynivalenol (DON) and 0.09 mg zearalenone (ZON) per kg dry matter) at different feed intake levels on the biotransformation and carry-over of DON in dairy cows. For this purpose, 14 ruminal and duodenal fistulated dairy cows were fed a diet containing 60% concentrate with a wheat portion of 55% (Fusarium toxin-contaminated wheat (mycotoxin period) or control wheat (control period)) and the ration was completed with maize- and grass silage (50 : 50) on a dry matter basis. Daily DON intakes ranged from 16.6 to 75.6 mg in the mycotoxin period at dry matter intakes of 5.6-20.5 kg. DON was almost completely biotransformed to de-epoxy DON (94-99%) independent of the DON/feed intake, and the flow of DON and de-epoxy DON at the duodenum related to DON intake ranged from 12 to 77% when the Fusarium toxin-contaminated wheat was fed. In the serum samples, de-epoxy DON was detected in the range of 4-28 ng ml-1 in the mycotoxin period, while concentrations of DON were all below the detection limit. The daily excretion of DON and de-epoxy DON in the milk of cows fed the contaminated wheat varied between 1 and 10 microg and between 14 and 104 microg, respectively. The total carry-over rates as the ratio between the daily excretion of DON and de-epoxy DON into milk and DON intake were in the ranges of 0.0001-0.0002 and 0.0004-0.0024, respectively. Total carry-over rates of DON as DON and de-epoxy DON into the milk increased significantly with increasing milk yield. In the urine samples, de-epoxy DON was the predominant substance as compared with DON with a portion of the total DON plus de-epoxy DON concentration to 96% when the Fusarium toxin-contaminated wheat was fed, whereas the total residues of DON plus de-epoxy DON in faeces ranged between 2 and 18% of DON intake in the mycotoxin period. The degree of glucuronidation of de-epoxy DON was found to be approximately 100% in serum. From 33 to 80% of DON and from 73 to 92% of de-epoxy DON, and from 21 to 92% of DON and from 86 to 100% of de-epoxy DON were glucuronidated in the milk and urine, respectively. It is concluded that DON is very rapidly biotransformed to de-epoxy DON in the rumen and only negligible amounts of DON and de-epoxy DON were transmitted into the milk within the range of 5.6-20.5 kg day-1 dry matter intake and milk yields (fat corrected milk) between 10 and 42 kg day-1.


Asunto(s)
Alimentación Animal/análisis , Bovinos/metabolismo , Contaminación de Alimentos/análisis , Tricotecenos/farmacocinética , Triticum/química , Animales , Biotransformación , Duodeno/metabolismo , Heces/química , Femenino , Análisis de los Alimentos/métodos , Fusarium , Leche/química , Tricotecenos/administración & dosificación , Tricotecenos/análisis
7.
Food Addit Contam ; 22(9): 864-74, 2005 Sep.
Artículo en Inglés | MEDLINE | ID: mdl-16192073

RESUMEN

As part of the certification campaign of three candidate reference materials for the determination of aflatoxin M1 (AfM1) in whole milk powders, homogeneity, short- and long-term stability tests of naturally contaminated milk powders have been performed. The homogeneity of two AfM1-contaminated milk powders was studied by taking samples at regular intervals of the filling sequences and analysing in triplicate for their AfM1 contents by liquid chromatography with fluorescence detection (LC-FLD) using random stratified sampling schemes. The homogeneity testing of an AfM1 'blank' milk powder material was performed by determining the nitrogen content because AfM1 levels were below the limit of detection of the most sensitive determination method. The short-term stability of AfM1-contaminated milk powders was evaluated at three different storage temperatures (4, 18 and 40 degrees C). After storage times of 0, 1, 2 and 4 weeks, samples were investigated using LC-FLD. The long-term stability study comprised of measurements after 0, 6, 12 and 18 months after storage at -20 and 4 degrees C. Analyses were done by LC-FLD. Based on the homogeneity tests, the materials were sufficiently homogenous to serve as certified reference materials. Corresponding uncertainty contributions of 0.23-0.89% were calculated for the homogeneity. The stability measurements showed no significant trends for both short- and long-term stability studies. The long-term stability uncertainties of the AfM1-contaminated milk powders were 7.4 and 6.3%, respectively, for a shelf-life of 6 years and storage at -20 degrees C. Supplementary stability monitoring schemes over a long period of several years are currently ongoing.


Asunto(s)
Aflatoxina M1/análisis , Contaminación de Alimentos/análisis , Leche/química , Animales , Bovinos , Análisis de los Alimentos/métodos , Análisis de los Alimentos/normas , Conservación de Alimentos/métodos , Humanos , Estándares de Referencia , Temperatura
8.
Anal Bioanal Chem ; 382(8): 1848-58, 2005 Aug.
Artículo en Inglés | MEDLINE | ID: mdl-16007445

RESUMEN

The lack of reliable, certified calibrant solutions for the Fusarium mycotoxins deoxynivalenol (DON), 3-acetyl-DON (3-Ac-DON), 15-acetyl-DON (15-Ac-DON) and nivalenol (NIV) is a serious drawback in the already problematic area of trichothecene analysis. For this reason, purified DON, 3-Ac-DON, 15-Ac-DON and NIV standards were processed, the conditions required for their isolation and purification were optimised, and the crystalline toxins were thoroughly characterised. Several complimentary analytical methods were used to evaluate the identities of the mycotoxins and the types and amounts of impurities; results obtained from 1H and 13C NMR spectra, as well as from IR-spectra, were in agreement with the literature. Elemental analysis revealed that the isolated NIV occurs as monohydrate. If this is not known it results in a weighing error of approximately 5%. Differential scanning calorimetry (DSC) was only successful for 15-Ac-DON, as the other trichothecenes decomposed during measurements. No traces of chloride, nitrate and sulphate were found by means of ion chromatography (IC). As expected UV absorption spectra for DON, NIV, 3-Ac-DON and 15-Ac-DON yielded lambda(max) values of 216, 217, 217 and 219 nm, respectively. Minor peaks due to impurities were observed by high performance liquid chromatography (HPLC) with UV detection. The main impurity peak in the DON sample was identified by LC-tandem mass spectroscopy (LC-MS/MS) as 4,7-dideoxy-NIV (7-deoxy-DON), which occurs at levels of approximately 1.4%. Gas chromatography (GC) was performed, coupled with either an electron capture detector (ECD), a flame ionisation detector (FID), or a mass spectrometric detector (MS); however, derivatisation prior to GC analysis makes the estimation of impurities difficult. LC-MS/MS was found to be unsuitable for quantifying levels of impurities. It can be concluded that high-purity (>97%) B-trichothecene standards were successfully processed and fully characterised for the first time.


Asunto(s)
Tricotecenos/análisis , Cromatografía Líquida de Alta Presión , Cromatografía Liquida , Espectroscopía de Resonancia Magnética , Espectrometría de Masas , Modelos Químicos , Espectrofotometría Ultravioleta
9.
Food Addit Contam ; 22(1): 48-55, 2005 Jan.
Artículo en Inglés | MEDLINE | ID: mdl-15895611

RESUMEN

Trichothecenes are mycotoxins produced by several fungal genera, mainly Fusarium species, that can contaminate a wide range of cereals used for human and animal consumption. They are associated with various adverse health effects in animals and humans such as feed refusal, vomiting and immunotoxic effects. A method based on capillary gas chromatography with mass spectrometric detection was developed and validated in-house for the determination of nine trichothecenes in duplicate diets of young children. The trichothecenes were extracted from the sample matrix by water/ethanol (90/10). The extracts were cleaned by means of ChemElut and Mycosep columns. The cleaned extracts were evaporated to dryness and derivatized to trimethylsilyl ethers at room temperature. The residues were dissolved in iso-octane and washed with water. The final extracts were analysed for trichothecenes by GC-MS. The response was linear in the range tested (1-10 microg kg(-1)). Recoveries for the trichothecenes were between 70 and 111%, with the exception of nivalenol, which had a low recovery (34%). The limit of quantification for all trichothecenes was below 0.4 microg kg(-1). Seventy-four food samples from young children collected by 74 respondents in a duplicate diet study were analysed for trichothecenes with the developed method. The mean levels of deoxynivalenol, nivalenol, HT-2 toxin and T-2 toxin were 5.8, 0.3, 0.3 and 0.1 microg kg(-1), respectively. Based on the individual results, dietary intake calculations were made. For deoxynivalenol, the tolerable daily intake of 1 microg kg(-1) body weight was exceeded by nine respondents. For the combined intake of T-2 and HT-2 toxin, the temporary tolerable daily intake of 0.06 microg kg(-1) body weight was exceeded by nine respondents.


Asunto(s)
Dieta , Contaminación de Alimentos/análisis , Tricotecenos/análisis , Peso Corporal , Grano Comestible/química , Análisis de los Alimentos/métodos , Cromatografía de Gases y Espectrometría de Masas/métodos , Humanos , Lactante , Tricotecenos/administración & dosificación
10.
Mycotoxin Res ; 21(1): 7-10, 2005 Mar.
Artículo en Inglés | MEDLINE | ID: mdl-23605197

RESUMEN

Within an EC-funded project calibrants with certified concentrations of Deoxynivalenol (DON), 3-Acetyl-Deoxynivalenol (3-Ac-DON), 15-Acetyl-Deoxynivalenol (15-Ac-DON) and Nivalenol (NIV) in acetonitrile have been produced. So far the project has led to improved isolation and purification of the solid toxins fromFusarium cultures. In addition, conditions for the production, ampouling and transport of the toxin solutions have been optimised. Further investigations should lead to knowledge about storage conditions and internationally accepted molar absorption coefficients for DON, 3-Ac-DON, 15-Ac-DON and NIV in acetonitrile. The intercomparison study which is currently carried out will also help to support knowledge and experience exchange between laboratories in the field ofFusarium mycotoxin analysis.

11.
Mycotoxin Res ; 21(4): 224-30, 2005 Dec.
Artículo en Inglés | MEDLINE | ID: mdl-23605392

RESUMEN

Within the EC-financed project "Feasibility Study for the Production of Certified Calibrants for the Determination of Deoxynivalenol and other B-Trichothecenes", an intercomparison study was performed with 13 European participants.Main goals of the intercomparison study were to check the feasibility of a small batch of gravimetrically prepared calibrants, to directly compare common and individually prepared calibrants, to test the practicability of toxin mixtures as calibrant solutions and finally to give recommendations for the means of certification. Additionally, it focused on the comparison of gas chromatography (GC) and high performance liquid chromatography (HPLC) for the determination of pure type-B trichothecene solutions, which is described in this publication.The participating laboratories received calibrant solutions as well as toxin solutions of unknown concentration and employed mainly HPLC-UV; GC-ECD (electron capture detection) and GC-MS (mass spectrometry) methods were used less often.The intercomparison study generally suffered from a high rate of outliers (22% of all the data). Throughout the study, 48% of all GC results were classified as outliers and it soon became apparent, that GC results highly infuenced the outcome of the study and that the used GC methods were not robust enough for the certification of type-B trichothecene calibrants. The high discrepancy between HPLC and GC results in the intercomparison study presumably lies in the crucial step of derivatisation.

12.
Food Addit Contam ; 21(4): 331-40, 2004 Apr.
Artículo en Inglés | MEDLINE | ID: mdl-15204557

RESUMEN

Paralytic shellfish poisoning toxins are produced by dinoflagellates. Shellfish filtering these unicellular algae will accumulate the toxins and pose a health risk when consumed by man. In the European Union, paralytic shellfish poisoning toxins in bivalve molluscs are regulated at a maximum content of 80 microg/100 g (91/492/EEC). The current reference method in the European Union is the mouse bioassay, but alternative methods including the liquid chromatography methodology are preferred for ethical reasons. Analyses of suspected shellfish batches revealed, however, unacceptable differences in results reported by a small group of Dutch laboratories all using liquid chromatography methods with precolumn derivatization, followed by fluorescence detection. Therefore, a series of proficiency studies were undertaken among these laboratories. In the first three studies, participants were more or less allowed their own choice of method execution details. This approach yielded unsatisfactory results. A fourth study was then initiated in which a standardized method was mandatory. Two types of test material were used in the fourth study: lyophilized Cardium tuberculatum material containing saxitoxin (STX) and decarbamoyl-saxitoxin (dc-STX), and lyophilized mussel material containing dc-STX. The latter material was investigated in an interlaboratory study involving 15 participants and was considered as the reference material. Among the four laboratories, coefficients of variation (ANOVA) for C. tuberculatum material were 10% (n = 11) and 9% (n = 12) for STX and dc-STX, respectively, and for the reference material was 8% (n = 12) for dc-STX. The joint efforts showed that variability in analysis results between laboratories that all apply more or less the same method can be drastically improved if the methodology is rigorously standardized.


Asunto(s)
Toxinas Marinas/análisis , Neurotoxinas/análisis , Saxitoxina/análogos & derivados , Mariscos/análisis , Cromatografía Liquida/métodos , Cromatografía Liquida/normas , Análisis de los Alimentos/métodos , Análisis de los Alimentos/normas , Humanos , Laboratorios/normas , Toxinas Marinas/aislamiento & purificación , Países Bajos , Neurotoxinas/aislamiento & purificación , Control de Calidad , Reproducibilidad de los Resultados , Saxitoxina/análisis , Saxitoxina/aislamiento & purificación
13.
J AOAC Int ; 84(5): 1668-76, 2001.
Artículo en Inglés | MEDLINE | ID: mdl-11601490

RESUMEN

A project was undertaken to develop mussel reference materials that were certified for their mass fractions of saxitoxin and decarbamoyl-saxitoxin. Fifteen laboratories from various European countries participated. Three of these had major responsibility for substantial parts of the work and overall coordination of the project. The project involved 4 main activities: (1) procurement and characterization of calibrants; (2) improvement of analytical methodology; (3) preparation of reference materials, including homogeneity and stability studies; (4) 2 interlaboratory studies and a certification exercise. The joint activities resulted in 3 homogeneous and stable reference materials: 2 lyophilized mussel materials with and without naturally incurred paralytic shellfish poisoning (PSP) toxins, and a saxitoxin enrichment solution. The reference materials were certified with respect to their saxitoxin and decarbamoyl-saxitoxin content. The lyophilized mussel material with PSP toxins (CRM 542) contained <0.07 mg saxitoxin x 2HCl/kg and 1.59 +/- 0.20 mg decarbamoyl-saxitoxin x 2HCl/kg. The lyophilized mussel material without PSP toxins (CRM 543) contained <0.07 mg saxitoxin x 2HCl/kg and <0.04 mg decarbamoyl-saxitoxin x 2HCl/kg. The certified value of the saxitoxin mass fraction in the saxitoxin enrichment solution (CRM 663) was 9.8 +/- 1.2 microg/g.


Asunto(s)
Bivalvos/química , Parálisis/inducido químicamente , Saxitoxina/análisis , Mariscos/análisis , Animales , Calibración , Certificación , Liofilización , Estándares de Referencia , Reproducibilidad de los Resultados , Saxitoxina/análogos & derivados
14.
Food Addit Contam ; 18(9): 810-24, 2001 Sep.
Artículo en Inglés | MEDLINE | ID: mdl-11552748

RESUMEN

This paper describes the second part of a project undertaken to develop certified mussel reference materials for paralytic shellfish poisoning toxins. In the first part two interlaboratory studies were undertaken to investigate the performance of the analytical methodology for several PSP toxins, in particular saxitoxin and decarbamoyl-saxitoxin in lyophilized mussels, and to set criteria for the acceptance of results to be applied during the certification exercise. Fifteen laboratories participated in this certification study and were asked to measure saxitoxin and decarbamoyl-saxitoxin in rehydrated lyophilized mussel material and in a saxitoxin-enriched mussel material. The participants were allowed to use a method of their choice but with an extraction procedure to be strictly followed. The study included extra experiments to verify the detection limits for both saxitoxin and decarbamoyl-saxitoxin. Most participants (13 of 15) were able to meet all the criteria set for the certification study. Results for saxitoxin.2HCl yielded a certified mass fraction of <0.07 mg/kg in the rehydrated lyophilized mussels. Results obtained for decarbamoyl-saxitoxin.2HCl yielded a certified mass fraction of 1.59+/-0.20 mg/kg. The results for saxitoxin.2HCl in enriched blank mussel yielded a certified mass fraction of 0.48 +/- 0.06 mg/kg. These certified reference materials for paralytic shellfish poisoning toxins in lyophilized mussel material are the first available for laboratories to test their method for accuracy and performance.


Asunto(s)
Bivalvos/química , Certificación/métodos , Contaminación de Alimentos , Saxitoxina/análisis , Animales , Liofilización/métodos , Humanos , Estándares de Referencia , Saxitoxina/análogos & derivados , Saxitoxina/química , España
16.
Food Addit Contam ; 17(6): 419-33, 2000 Jun.
Artículo en Inglés | MEDLINE | ID: mdl-10932785

RESUMEN

This paper describes the first part of a project undertaken to develop mussel reference materials for Paralytic Shellfish Poisoning (PSP) toxins. Two interlaboratory studies were undertaken to investigate the performance of the analytical methodology for several PSP toxins, in particular saxitoxin (STX) and decarbamoyl-saxitoxin (dc-STX) in lyophilized mussels, and to set criteria for the acceptance of results to be applied during the second part of the project: the certification exercise. In the first study, 18 laboratories were asked to measure STX and dc-STX in rehydrated lyophilized mussel material and to identify as many other PSP toxins as possible with a method of their choice. In the second interlaboratory study, 15 laboratories were additionally asked to determine quantitatively STX and dc-STX in rehydrated lyophilized mussel and in a saxitoxin-enriched mussel material. The first study revealed that three out of four post-column derivatization methods and one pre-column derivatization method sufficed in principle to determine STX and dc-STX. Most participants (13 of 18) obtained acceptable calibration curves and recoveries. Saxitoxin was hardly detected in the rehydrated lyophilized mussels and results obtained for dc-STX yielded a CV of 58% at a mass fraction of 1.86 mg/kg. Most participants (14 out of 18) identified gonyautoxin-5 (GTX-5) in a hydrolysed extract provided. The first study led to provisional criteria for linearity, recovery and separation. The second study revealed that 6 out of 15 laboratories were able to meet these criteria. Results obtained for dc-STX yielded a CV of 19% at a mass fraction of 3.49 mg/kg. Results obtained for STX in the saxitoxin-enriched material yielded a CV of 19% at a mass fraction of 0.34 mg/kg. Saxitoxin could not be detected in the PSP-positive material. Hydrolysis was useful to confirm the identity of GTX-5 and provided indicative information about C1 and C2 toxins in the PSP-positive material. The methods used in the second interlaboratory study showed sufficiently consistent analysis results to undertake a certification exercise to assign certified values for STX and dc-STX in lyophilized mussel.


Asunto(s)
Bivalvos/química , Toxinas Marinas/análisis , Neurotoxinas/análisis , Mariscos/análisis , Animales , Liofilización , Laboratorios/normas , Toxinas Marinas/normas , Estructura Molecular , Neurotoxinas/química , Neurotoxinas/normas , Estándares de Referencia , Saxitoxina/análogos & derivados , Saxitoxina/análisis , Mariscos/normas
17.
Food Chem Toxicol ; 38(8): 679-88, 2000 Aug.
Artículo en Inglés | MEDLINE | ID: mdl-10908815

RESUMEN

The dietary subacute toxicity of the ergot alkaloid alpha-ergocryptine was studied in Sprague-Dawley rats. Rats were fed 0, 4, 20, 100 or 500 mg ergocryptine/kg diet for 28-32 days (equal to 0, 0.36, 1.7, 8.9 and 60 mg ergocryptine/kg body weight/day for females and 0, 0.34, 1.4, 6.6 and 44 mg ergocryptine/kg body weight/day for males). The present study describes the general toxicological effects; the effects on metabolic and hormonal parameters will be reported separately. Body weight, body weight gain, food intake and food efficiency were all decreased with a U-shaped dose-response curve, as in both sexes the ranking severity of effects was in the order 100-20-500 and 4 mg/kg diet. Other changes with a U-shaped dose-response relationship included: hematological parameters (decreased MCV and MCH), serum enzyme activities (slightly increased/decreased ALAT, ASAT, GGT), increased serum urea concentrations, decreased glomular filtration (creatinine and urea clearances), decreased absolute organ weights, increased and decreased relative organ weights, atrophy of thymus and in females atrophy of ovary and uterus with in the mid-dose groups no detectable morphological features of an oestric cycle in the uterus. Other parameters, including increased relative liver, heart and ovarian weights and necrosis of the tail, were influenced in a dose-related manner or only in the high dose group. The U-shaped changes for the parameters mentioned above might be caused by the U-shaped dose-response relationship for food intake, which may be explained by the dopaminergic properties of alpha-ergocryptine. It is concluded that in rats fed ergocryptine for 28 days the dose-effect curve is rather steep and that the NOAEL is 4 mg/kg diet.


Asunto(s)
Agonistas de Dopamina/toxicidad , Ergolinas/toxicidad , Animales , Peso Corporal/efectos de los fármacos , Pruebas de Química Clínica , Relación Dosis-Respuesta a Droga , Ingestión de Alimentos/efectos de los fármacos , Metabolismo Energético/efectos de los fármacos , Estro/efectos de los fármacos , Femenino , Masculino , Nivel sin Efectos Adversos Observados , Tamaño de los Órganos/efectos de los fármacos , Ratas , Ratas Sprague-Dawley , Aumento de Peso/efectos de los fármacos
18.
Food Addit Contam ; 15(4): 385-8, 1998.
Artículo en Inglés | MEDLINE | ID: mdl-9764206

RESUMEN

Seventy-eight maize-containing foods obtained from retail stores in The Netherlands were analysed for fumonisin B1 contamination. Thirty-six per cent of the samples were contaminated with fumonisin B1 in the range of 8 micrograms kg-1 (limit of detection) to 1430 micrograms/kg-1. Forty-six per cent of the minimally treated maize samples (n = 39; maize for bread production, maize for popcorn, maize flour and polenta) were contaminated with fumonisin B1 in the range of 8-380 micrograms kg-1. Twenty-six per cent of the maize-containing processed foods (n = 39; tostada, canned maize, maize starch, maize bread, popped maize, flour mixes, maize chips and cornflakes) were contaminated with fumonisin B1 in the range of 8-1430 micrograms/kg-1. This survey shows that maize-containing foods in The Netherlands frequently can be contaminated with fumonisin B1.


Asunto(s)
Ácidos Carboxílicos/análisis , Carcinógenos Ambientales/análisis , Exposición a Riesgos Ambientales , Contaminación de Alimentos/análisis , Fumonisinas , Teratógenos/análisis , Zea mays , Pan/análisis , Humanos , Países Bajos
19.
Food Addit Contam ; 15(4): 389-92, 1998.
Artículo en Inglés | MEDLINE | ID: mdl-9764207

RESUMEN

Sixty-two samples of maize imported in The Netherlands and intended for human consumption were screened for the presence and concentration of fumonisin B1. Sixty-one of those samples contained fumonisin B1 with concentrations ranging from 30 to 3350 micrograms kg-1, 11 maize samples contained > 1000 micrograms kg-1. The average fumonisin B1 concentration was 640 micrograms kg-1 for the positive samples and 620 micrograms kg-1 for all samples. Medians were 600 micrograms kg-1 and 550 micrograms kg-1 for positive and all samples, respectively. The results obtained were comparable to results from other studies in maize from various countries.


Asunto(s)
Ácidos Carboxílicos/análisis , Carcinógenos Ambientales/análisis , Contaminación de Alimentos/análisis , Fumonisinas , Zea mays/química , Cromatografía Líquida de Alta Presión , Industria de Procesamiento de Alimentos , Humanos , Países Bajos
20.
J Food Prot ; 61(7): 879-84, 1998 Jul.
Artículo en Inglés | MEDLINE | ID: mdl-9678173

RESUMEN

Fumonisin B1 is currently regarded as the most significant mycotoxin produced by Fusarium spp. It has carcinogenic properties and may play a role in the etiology of human esophageal cancer. The human population is exposed to fumonisin B1 primarily by intake of fumonisin B1-contaminated maize. Maize consumed in the Netherlands is imported from all parts of the world. Since processing will not affect the overall toxic effect, the fumonisin B1 intake is directly related to the quantity of maize consumed. Literature results concerning the occurrence of fumonisin B1 in a total of 349 samples of maize from 18 countries worldwide demonstrated the presence of this mycotoxin in 93% of the samples. The median fumonisin B1 contamination of all samples was 420 ng of fumonisin B1 per g of maize, and the average contamination level was 1,359 ng of fumonisin B1 per g of maize. Human intake of fumonisin B1 was estimated based on the maize consumption of all people in the Netherlands in 1992. A probability distribution was derived to allow estimation of the exposure of the population to fumonisin B1 intake in relation to maize intake. It showed that among those in the group considered to be at risk, people with gluten intolerance such as people with celiac or Dühring's disease, 37% are estimated to be exposed to an intake of at least 10(5) ng and 97% to an intake of at least 10(3) ng of fumonisin B1 per person per day. For all people in the Netherlands these percentages would be 1% and 49%, respectively.


Asunto(s)
Ácidos Carboxílicos/análisis , Fumonisinas , Micotoxinas/análisis , Zea mays/microbiología , Ácidos Carboxílicos/administración & dosificación , Ácidos Carboxílicos/toxicidad , Humanos , Países Bajos , Gestión de Riesgos , Zea mays/química
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